Spectroscopic analysis of roman wall paintings from Casa del Mitreo in Emerita Augusta, Mérida, Spain

The use of visible spectroscopy, applied to chromatic characterization of Roman wall paintings, allows an easy and trustworthy grouping of the samples studied. The use of other spectroscopic techniques such as Fourier transform infrared spectroscopy (FTIR) and energy-dispersive X-ray spectroscopy (EDS) in conjunction with X-ray diffraction (XRD) allows a good identification of the substances present in the pictorial layers that define and differentiate each chromatic group. In this paper, a study of 40 Roman wall painting samples, from Pinturas Báquicas of Casa del Mitreo in Emerita Augusta (Mérida, Spain), is described. In these samples, some pigments of high quality and cost, as well as some unusual mixtures, not described in the bibliography, have been found.     

An overview of the analytical characterization of nanostructured drug delivery systems: Towards green and sustainable pharmaceuticals: A review

The analytical characterization of drug delivery systems prepared by means of green manufacturing technologies using CO₂ as a processing fluid is here reviewed. The assessment of the performance of nanopharmaceuticals designed for controlled drug release may result in a complex analytical issue and multidisciplinary studies focused on the evaluation of physicochemical, morphological and textural properties of the products may be required. The determination of the drug content as well as the detection of impurities and solvent residues are often carried out by chromatography. Assays on solid state samples relying on X-ray, vibrational and nuclear magnetic resonance spectroscopies are of great interests to study the composition and structure of pharmaceutical forms. The morphology and size of particles are commonly checked by microscopy and complementary chemical information can be extracted in combination with spectroscopic accessories. Regarding the thermal behavior, calorimetric and thermogravimetric techniques are applied to assess the thermal transitions and stability of the samples. The evaluation of drug release profiles from the nanopharmaceuticals can be based on various experimental set-ups depending on the administration route to be considered. Kinetic curves showing the evolution of the drug concentration as a function of time in various physiological conditions (e.g., gastric, plasmatic or topical) are recorded commonly by UV–vis spectroscopy and/or chromatography. Representative examples are commented in detail to illustrate the characterization strategies.     

Methodology for determination of magnetic force of polymeric nanocomposites

Magnetic nanocomposites present several interesting uses. They are very useful in environmental recovery, drug delivery and sensor applications. However, sophisticated magnetic measurements are very complex and present high costs, which may sometimes prevent research on these materials. Therefore, this paper presents a magnetic force test, which can be performed at relatively low cost and produces interesting results, which are very useful to support the development of these magnetic materials. Specifically, polylactic acid (PLA)/maghemite nanocomposites were prepared and characterized using Fourier transform infrared (FTIR) spectroscopy, wide-angle X-ray scattering (WAXS), small-angle X-ray scattering (SAXS) and size-exclusion chromatography (SEC). Our results demonstrate that nanocomposites, were obtained, which were also subjected to the magnetic force and magnetic susceptibility tests. The results of these latter tests were found to be linearly related, which proves the utility of the magnetic force test as a practical characterization technique.     

Characterization of green copper phase pigments in Egyptian artifacts with X-ray absorption spectroscopy and principal components analysis

The characterization of materials in historical artifacts can contribute significantly to their preservation and understanding; however, sampling and characterization are ideally performed using non-destructive approaches. The analysis of green pigments from Egyptian artifacts presents a further challenge as responses to laboratory based techniques have proven unsuccessful in many cases. An alternative approach is the use of non-destructive X-ray absorption near-edge structure spectroscopy, which was performed on a reference set of copper-containing green minerals and other compounds. Data projection using principal component analysis was used to explore the spectral data structures and to illustrate the relationship between the spectra and copper speciation, resulting in a calibration or training set of the reference materials used. Data from the training set were compared with samples from Egyptian artifacts. The combination of X-ray absorption spectroscopy with principal components analysis provides a novel approach in archeometry and the characterization of objects of cultural heritage.     

Development of a combined method to carry out a multielement analysis for environment preser vation

The paper discusses the possibilities of energy dispersive X-ray fluorescence spectroscopy and instrumental neutron activation analysis in the investigation of environmental pollutions. The X-ray fluorescence spectroscopy of samples was performed using the MECA-1044A analyzer (XR-500, LINC SYSTEMS, Great Britain) with a pulsed X-ray tube with a silver target as a source of excitation. Neutron activation analysis was carried out on the basis of two reactors: IBR-2 LNP JINR, Dubna, and TWR ITEP, Moscow. The optimal regimes of measurement for both methods as well as the detection limits corresponding to these regimes are given. To illustrate the perspectives of the methods, the ecological problem of the consequences of introducing into soil of the now available meliorator CaSO₄·2H₂O is solved in the paper. Data on absorption of trace elements in a wide range including rare-earth elements by agricultural plants are presented. This paper may be of interest for specialists in analytical chemistry and ecology.     

Major element analysis of selected rock and volcanic ash samples in the Unzen area,Japan, by X-ray fluorescence spectroscopy

Determination of major elements in natural solid samples by X-ray fluorescence spectroscopy (XRF) with a fusion disc technique is described. Data obtained by the present XRF analytical system were found to have satisfactorily high reliability. Five rock samples and a volcanic ash sample with varying ages ranging from the present to 180 000 years, derived by the current and past volcanic activities in the Unzen area, Nagasaki, Japan were analyzed for their major elements' compositions using the above mentioned system. The chemical composition of the magma under this area has changed very little at least over the last 180 000 years.     

Preparation by different methods and analytical characterization of gadolinium-doped ceria

The present work reports the influence of chemical synthesis on structural, morphological and optical properties of gadolinium-doped ceria (GDC) with analytical characterization of synthesized specimens. GDC powders with Gd content of 10, 15 and 20 mol% were synthesized by aqueous sol–gel and sol–gel combustion methods using glycerol as complexing agent and fuel. The phase purity and structural features of obtained powders were evaluated using X-ray diffraction analysis and Raman spectroscopy. These studies confirmed that crystallization of GDC occurs into cubic fluorite-type crystal structure. Morphological features as well as optical properties of GDC powders were determined to be strongly dependent on the synthesis method. To confirm chemical composition of prepared samples, spectrophotometric approach for the determination of Ce and Gd in GDC samples was suggested. Relative standard deviation values for Ce and Gd were in the range of 1.5–4.1 and 2.0–5.6%, respectively. The obtained results demonstrated that the suggested analytical procedure can be successfully used for the analysis of GDC specimens with high accuracy.     

Green Synthesis and Characterization of Zinc Oxide Using Carica papaya Leaf Extract

Environmental methodologies are gaining recognition in this modern world. Environmental nanotechnology plays a major role in improving modern fields of environmental engineering and science. Metal oxide nanoparticles have exceptional properties due to their small size, including quantum confinement, surface-to-volume ratio, plasmon excitation, high biocompatibility, and surface modifiability. The biosynthesis of nanoparticles using fungi, bacteria, and plants through various biotechnological techniques is currently a new paradigm for environmental protection. Synthesis of nanoparticles through plant extract is good because it eliminates the dangers of toxic chemicals, it is environmentally friendly, simpler, and safer as the reaction time is reduced and it can also be increased in size for higher operation. The present study is based on the development of zinc oxide nanoparticles from papaya leaf extract where zinc nitrate is used as a precursor. The biosynthesized nanoparticles are characterized by X-ray diffraction, Fourier transform infrared spectroscopy, electron microscopy, energy-dispersive X-ray analysis, UV-visible spectroscopy, and dynamic light scattering analysis. The crystalline phase determination of the zinc oxide nanoparticles is analyzed by X-ray diffraction and the formation of polycrystalline zinc oxide nanoparticles is confirmed. FT-IR spectrum reveals the main functional groups and chemical information in zinc oxide nanostructures. Morphological analysis is performed using SEM at different magnification levels. EDAX analysis shows the purity of the composite samples. Optical characterization is performed using a UV–vis spectrophotometer. DLS analysis shows that the nanoparticles formed have a relatively well-defined dimension.     

Superhard coatings — Production and analysis

In the development of diamond and c-BN products the analytical methods for characterizing the surface, bulk and interface of the diamond coatings are very important. SEM, Raman, XRD and IR are the methods used for characterization and SIMS, TEM, AES, NRA, RBS, XPS, STM, etc. are used for the investigation of special problems. The techniques for diamond and c-BN production are briefly summarized to give an idea of the complex interactions between production, application and analytical characterization. The analytical methods for diamond characterization and many relevant results are summarized in this paper; some physical properties (e.g. thermal conductivity, transparency, etc.) and their interaction with applications are also discussed.Abbreviations AES Auger electron spectroscopy - AFM atomic force microscopy - c-BN cubic boron nitride - CL cathodoluminescence - CVD chemical vapour deposition - EELS electron energy loss spectroscopy - EPMA electron probe microanalysis - ERDA elastic recoil detection analysis - h-BN hexagonal boron nitride - HP-HT high-pressure high-temperature - HF hot-filament - IR infra-red - LEED low energy electron diffraction - MW microwave - NAA neutron activation analysis - NRA nuclear reaction analysis - PL photoluminescence - PVD physical vapour deposition - RBS Rutherford backscattering spectrometry - RHEED reeflected high energy electron diffraction - SAD selected area diffraction - SEM scanning electron microscopy - SIMS secondary ion mass spectrometry - STM secondary ion mass spectrometry - TEM transmission electron microscopy - TMB trimethylborate - XPS X-ray photoelectron spectroscopy - XRD X-ray diffraction Dedicated to Professor Dr. rer. nat. Dr. h.c. Hubertus Nickel on the occasion of his 65th birthday     

Preparation and characterization of a Mexican organo clinoptilolite-heulandite mineral and its evaluation for the sorption of cadmium and cobalt

The preparation and characterization of a Mexican organo clinoptilolite-heulandite mineral as well as the evaluation of its sorption properties for cadmium and cobalt are presented. The mineral was modified with different concentrations of hexadecyltrimethyl-ammonium bromide (HDTMA), the resulting materials were characterized by electron microscopy, IR spectroscopy, BET surface analysis, X-ray diffraction and their cation exchange capacities were determined. The cobalt and cadmium uptake was carried out in different concentrations. Neutron activation was used to measure the sorption of cobalt and cadmium. Organo zeolitic mineral samples were obtained with different surface characteristics compared with the original material and it was found that the retention of cobalt and cadmium by the organo zeolite diminishes due to the presence of HDTMA.     

Structure of red and orange fluorescein

The structures of colorless, red, and yellow-orange fluorescein have been investigated by a combination of solution and solid state¹³C NMR. It is demonstrated that the three forms have lactonic, zwitterionic, and quinoid structures, respectively. Conflicting X-ray, NMR, and IR structural evidence is discussed for samples of red fluorescein which cannot readily be obtained in definite crystalline form. It is concluded that solid-state¹³C NMR spectroscopy is superior by revealing primarily the molecular structure but being fairly insensitive toward lattice variations.The Editors regret the long delay in having this paper printed due to an unfortunate administrative error.     

金属组学：高通量分析技术进展与展望

金属组学是系统研究一种细胞、组织或完整生物体内全部金属原子的分布、含量、化学种态及其功能的新兴综合学科,它的提出受到人们越来越多的关注。本文综述了金属组学的研究方法,并对各种方法的特点和局限性做了比较说明．ICP-MS与NAA技术可实现多元素同时定量分析,同步辐射微束CT及μRF,EDX,PIXE,SIMS及LA-ICP—MS亦可实现金属组分布研究．金属组学研究目前正处于发展初期,仍有许多困难特别是分析仪器及方法方面的问题有待解决．已有的金属组形态及结构分析工作大多数采用的是较低效率的分析方法,一些正在发展中的关键技术平台,如HTXAS可真正实现高通量的形态或结构分析．此外,生物信息学有望成为金属组学研究的重要工具之一．     

Noninvasive methods for the investigation of ancient Chinese jades: an integrated analytical approach

This paper reports on an integrated analytical approach for the noninvasive characterization of Chinese nephrite samples, encompassing both geological reference specimens and museum objects. Natural variations induced by cationic substitutions, as well as human-induced alterations such as heating, which both affect color, are the focus of this contribution. Totally noninvasive methods of analysis were used, including X-ray fluorescence spectroscopy, Raman microspectroscopy, visible reflectance spectroscopy and X-ray diffraction; moreover, the feasibility of using a portable Raman spectrometer for the in-field identification of jades has been demonstrated. Fe/Fe+Mg (% p.f.u.) ratios of the jades have been calculated based on hydroxyl stretching Raman bands, which will provide an important addition to similar data that are being collected at major museums in the Western and Eastern hemispheres.      

Hg diffusion in books of XVIII and XIX centuries by synchrotron microprobe

The pigment vermilion (HgS) was used to color the fore edge, tail and head of books. Dissemination and quantification of Hg present in the ink used to color books from XVIII and XIX centuries are reported. Mercury is a very toxic element for the human body, therefore it is extremely important to know whether Hg tends to disseminate throughout the paper or stays confined to the borders of the books with less danger for readers. Synchrotron X-ray microprobe was used to evaluate Hg dissemination from the border to the centre of the paper sheet. The diffusion pattern of Hg was compared with the results obtained by a portable X-ray fluorescence spectrometer and mean quantitative calculations were obtained by a stationary X-ray fluorescence system with triaxial geometry. The results showed high concentrations of Hg in the external regions, but no diffusion was observed for the inner parts of the paper.     

Analytical techniques for characterization of organic molecular assemblies in molecular electronics devices

The analytical techniques used for the physical characterization of organic molecular electronic-based devices are surveyed and discussed. These protocols include methods that are used to probe molecular assemblies such as single wavelength ellipsometry, water contact angle goniometry, cyclic voltammetry, infrared spectroscopy, and X-ray photoelectron spectroscopy, and methods used to measure charge transport properties of devices such as scanning tunneling microscopy, and inelastic electron tunneling spectroscopy. Examples from our laboratory and the literature are given for each of these analytical techniques.     

Nanosphere lithography: fabrication of large-area Ag nanoparticle arrays by convective self-assembly and their characterization by scanning UV-visible extinction spectroscopy

This work employs UV-visible extinction spectroscopy as a new spectral mapping technique to characterize self-assembled polystyrene microsphere samples produced by convective self-assembly (CSA). This spectroscopic technique was successfully used to analyze the periodic particle arrays produced by the polystyrene template, yielding a detailed characterization of each sample. The CSA-prepared samples proved to be more uniform across a sample as well as more reproducible than previous sample preparation techniques. For the first time, a detailed characterization and quantitative evaluation of the entire sample has been performed by spectroscopic mapping.     

Compositional and electrochemical characterization of noble metal-diamondlike carbon nanocomposite thin films

A detailed characterization of platinum- and gold-diamondlike carbon (DLC) nanocomposite films deposited onto silicon substrates is presented. A modified pulsed laser deposition (PLD) technique was used to incorporate noble metal nanoclusters into hydrogen-free DLC films. Several analytical techniques, including transmission electron microscopy, atomic force microscopy, Rutherford backscattering spectroscopy, X-ray photoelectron spectroscopy, Raman spectroscopy, and nanoindentation testing, were used to investigate these thin films in an effort to determine their physical and electrochemical properties. Rutherford backscattering spectroscopy indicated that the gold- and platinum-DLC films contain metal concentrations between three and 36 atomic percent. Cross-sectional transmission electron microscopy revealed that metal is present as arrays of noble metal islands embedded within the DLC matrix, while atomic force microscopy provided evidence of target splashing. In addition, due to the inclusion of metal, metal-DLC thin films exhibited greater conductivity than their metal-free counterparts. The electrochemical properties were studied using quasi-reversible redox couples and correlated to the metal concentration. Finally, the influence of the layer's composition on the electron-transfer kinetics and the achievable working potential window is discussed. The results discussed herein suggest that metal-DLC thin films grown by pulsed laser deposition present a promising alternative electrode material for electrochemistry.     

Multiscale characterization and constitutive parameters identification of polyamide (PA12) processed via selective laser sintering

This study is focused on multiscale characterization and constitutive parameters identification of selectively laser sintered PA12 specimens. The process parameters and change in crystallinity due to 3D printing were identified via differential scanning calorimetry (DSC). Tension, compression, shear, flexural and fracture tests performed on samples fabricated, both in 0° and 90° directions reveal that the tensile toughness of samples printed in 0° orientation, outperform samples printed in 90° orientation by an average of 24%. Cryogenically fractured samples were analyzed via SEM and micro-computed tomography to analyze 2D/3D defects and correlate the microstructure with macroscopic properties. The constitutive parameters for a strain-rate and temperature-dependent Three Network (TN) material model were identified using the measured mechanical properties. Furthermore, mechanical response of micro-architected Kelvin lattice structure was analyzed by Finite Element Method employing the TN constitutive model and the predictions were corroborated with measurements.     

Characterization of small particles by micro X-ray fluorescence

Micro X-ray fluorescence was used to study both homogeneous and heterogeneous particle systems. Specifically, homogeneous glass microspheres and heterogeneous soil particle samples were prepared by both bulk and single particle sample preparation methods for evaluation by micro X-ray fluorescence. Single particle sample preparation methods allow for single particles from a collected sample to be isolated and individually presented to the micro X-ray fluorescence instrument for analysis. Various particle dispersion methods, including immobilization onto Tacky Dot™ slides, mounting onto double-sided sticky tape affixed to polypropylene film, or attachment to polypropylene film using 3M Artist's Adhesive, were used to separate the sample particles for single particle analysis. These methods were then compared and evaluated for their ability to disperse the particles into an array of single separated particles for optimal micro X-ray fluorescence characterization with minimal background contribution from the particle mounting surface. Bulk methods of particle sample preparation, which included pellet preparation and aerosol impaction, used a large quantity of collected single particles to make a single homogeneous specimen for presentation to the instrument for analysis. It was found that single particle elemental analysis by micro X-ray fluorescence can be performed if the particles are well separated (minimum separation distance = excitation source beam diameter) down to a particle mass of ∼ 0.04 ng and a mean particle diameter of ∼ 0.06 μm. Homogeneous particulates can be adequately characterized by micro X-ray fluorescence using either bulk or single particle analysis methods, with no loss of analytical information. Heterogeneous samples are much harder to characterize, and both single particle as well as bulk analyses must be performed on the sample to insure full elemental characterization by micro X-ray fluorescence.